Improvement of the mechanical properties of SiC reticulated porous ceramics with optimized three-layered struts for porous media combustion

Silicon carbide reticulated porous ceramics (SiC RPCs) with three-layered struts were fabricated by polymer replica method, followed by infiltrating alumina slurries containing silicon (slurry-Si) and andalusite (slurry-An), respectively. The effects of composition of infiltration slurries on the strut structure, mechanical properties and thermal shock resistance of SiC RPCs were investigated. The results showed that the SiC RPCs infiltrated with slurry-Si and slurry-An exhibited better mechanical properties and thermal shock resistance in comparison with those of alumina slurry infiltration, even obtained the considerable strength at 1300 °C. In slurry-Si, silicon was oxidized into SiO₂ in the temperature range from 1300 °C to 1400 °C and it reacted with Al₂O₃ into mullite phase at 1450 °C. Meantime, the addition of silicon in slurry-Si could reduce SiC oxidation of SiC RPCs during firing process in contrast with alumina slurry. With regard to slurry-An, andalusite started to transform into mullite phase at 1300 °C and the secondary mullitization occurred at 1450 °C. The enhanced mechanical properties and thermal shock resistance of SiC RPCs infiltrated alumina slurries containing silicon and andalusite were attributed to the optimized microstructure and the triangular zone (inner layer of strut) with mullite bonded corundum via reaction sintering. In addition, the generation of residual compressive stress together with better interlocked needle-like mullite led to the crack-deflection in SiC skeleton, thus improving the thermal shock resistance of obtained SiC RPCs.     

A novel design of Al2O3-ZrO2 reticulated porous ceramics with hierarchical pore structures and excellent properties

The use of reticulated porous ceramics(RPCs) was of great interest in high-temperature catalytic application owing to their high surface area. In order to further optimize the pore structure and mechanical properties of RPCs, vacuum infiltration with CaCO₃-Al₂O₃ slurries process was applied to fabricate Al₂O₃-ZrO₂ RPCs with hierarchical pore structures. The pores within ceramic struts were prepared by processes of CaCO₃ decomposition and calcium hexaluminate grains growth. And the compressive residual stress was formed within multi-layered struts owing to the difference in the thermal expansion of coating layer and ceramic struts, which was established as a key factor in improving the mechanical properties and thermal shock resistance of RPCs. Furthermore, the size of pores within struts ranging from 5 μm to 14 μm affected the thermal shock resistance of RPCs significantly based on grey incidence analysis. And the potential of this materials as high-temperature catalyst supports was demonstrated.     

A nitride whisker template for growth of mullite in SiC reticulated porous ceramics

Silicon carbide reticulated porous ceramics (SiC RPCs) were fabricated by polymer replica technique. The effects of nitride whisker template on the growth of mullite, the strut structure and mechanical properties of SiC RPCs were investigated. Prepolyurethane (PU) open-cell sponge was first coated by SiC slurry consisting of SiC, reactive Al₂O₃, microsilica and Si powder, then it was nitridized at 1400 °C in a flowing N₂ atmosphere to prepare SiC preforms. Subsequently, these preforms were treated by vacuum infiltration of alumina slurry and fired at 1450 °C in air. The results showed that Si₂N₂O whiskers grew on the surface and in the matrix of SiC preforms after nitridation. The diameter of struts in SiC RPCs increased after vacuum infiltration process because alumina slurry was easily adhered by the surface nitride whiskers. In addition, such whiskers inside the strut of SiC preforms acted as the template to promote the growth of column-liked mullite in SiC RPCs. The mechanical properties and thermal shock resistance of SiC RPCs were greatly improved due to the special interfacial characteristics of multi-layered struts as well as better interlocked column-liked mullite in SiC skeleton.     

Fabrication of SiC reticulated porous ceramics with multi-layered struts for porous media combustion

Silicon carbide reticulated porous ceramics (SiC RPCs) with multi-layered struts were fabricated at 1450 °C by polymer sponge replica technique, followed by vacuum infiltration. The effect of additives (polycarboxylate, ammonium lignosulfonate and sodium carboxymethyl-cellulose) on the rheological behavior of silicon carbide slurry was firstly investigated, and then the slurry was coated on polyurethane open-cell sponge template. Furthermore, alumina slurry was adopted to fill up the hollow struts in vacuum infiltration process after the coated sponge was pre-treated at 850 °C. The results showed that the coating thickness on the struts and the microstructure in SiC RPCs were closely associated with the solid content of alumina slurry during vacuum infiltration. The typical multi-layered strut of SiC RPCs could be achieved after the infiltration of an alumina slurry containing 77 wt% solid content. The compressive strength and thermal shock resistance of the infiltrated specimens were significantly improved in comparison with those of non-infiltrated ones. The improvement was attributed to the in-situ formation of reaction-bonded multilayer struts in SiC RPCs, which were characterized by the exterior coating of aluminosilicate-corundum, middle part of mullite bonded SiC and interior zone of corundum.     

Preparation of SiC/SiC composites with high toughness by reaction of the SiCP+C double-cladding layer with liquid silicon

SiC/SiC composites prepared by liquid silicon infiltration (LSI) have the advantages of high densification, matrix cracking stress and ultimate tensile strength, but the toughness is usually insufficient. Relieving the residual microstress in fiber and interphase, dissipating crack propagation energy, and improving the crystallization degree of interphase can effectively increase the toughness of the composites. In this work, a special SiC particles and C (SiC_P +C) double-cladding layer is designed and prepared via the infiltration of SiC_P slurry and chemical vapor infiltration (CVI) of C in the porous SiC/SiC composites prepared by CVI. After LSI, the SiC generated by the reaction of C with molten Si combines with the SiC_P to form a layered structure matrix, which can effectually relieve residual microstress in fiber and interphase and dissipate crack propagation energy. The crystallization degree of BN interphase is increased under the effects of C-Si reaction exotherm. The as-received SiC/SiC composites possess a density of 2.64 g/cm³ and a porosity of 6.1%. The flexural strength of the SiC/SiC composites with layered structure matrix and highly crystalline BN interphase is 577 MPa, and the fracture toughness reaches up to 37 MPa·m^1/2. The microstructure and properties of four groups of SiC/SiC composites prepared by different processes are also investigated and compared to demonstrate the effectiveness of the SiC_P +C double-cladding layer design, which offers a strategy for developing the SiC/SiC composites with high performance.     

Mechanical Properties of Three-Layered Monolithic Silicon Nitride–Fibrous Silicon Nitride/Boron Nitride Monolith

A three-layered composite, composed of a strong outer layer (monolithic S₃N₄) and a tough inner layer (fibrous Si₃N₄/BN monolith), was fabricated by hot-pressing. For the inner layer, a Si₃N₄–polymer fiber made by extrusion was coated by dipping it into a 20 wt% BN-containing slurry. The three-layered composite exhibited excellent mechanical properties, including high strength, work of fracture, and crack resistance, because of the combination of a strong outer layer and a tough inner layer. In other words, the strong outer layer withheld the applied stress, while the tough inner layer promoted crack interactions through the weak BN cell boundaries. Also, the residual thermal stress on the surface due to the anisotropy in the coefficient of thermal expansion of BN affected a median/radial crack generation after indentation.     

Effects of heat treatment on the mechanical properties at elevated temperatures of plain-woven SiC/SiC composites

The effects of heat treatment on the mechanical properties of plain-woven SiC/SiC composites at 927 °C and 1200 °C in argon were evaluated through tensile tests at room temperature and at elevated temperature on the as-received and heat-treated plain-woven SiC/SiC composites, respectively. Heat treatment can improve the mechanical properties of composites at room temperature due to the release of thermal residual stress. Although heat treatment can damage the fiber, the effect of this damage on the mechanical properties of composites is generally less than the effect of thermal residual stress. Heat treatment will graphitize the pyrolytic carbon interface and reduce its shear strength. Testing temperature will affect the expansion or contraction of the components in the composites, thereby changing the stress state of the components. This study can provide guidance for the optimization of processing of ceramic matrix composites and the structural design in high-temperature environments.     

Residual Stress and Biaxial Strength in Sc2O3–CeO2–ZrO2/Y2O3–ZrO2 Layered Electrolytes

Multi‐layered (Y₂O₃)_0.08(ZrO₂)_0.92/(Sc₂O₃)_0.1(CeO₂)_0.01‐(ZrO₂)_0.89(YSZ/SCSZ) electrolytes have been designed, so that the inner SCSZ layers provided superior ionic conductivity and the outer YSZ skin layers maintained good chemical and phase stability. Due to the mismatch of coefficients of thermal expansion between layers of different compositions, the thermal residual stresses were generated. The theoretical residual stress and strain were calculated for different thickness ratios of the electrolytes. In order to study the residual stress effect on the mechanical properties, the biaxial flexure tests of electrolytes with various layered designs were performed via a ring‐on‐ring method at room temperature and 800 °C. The maximum principal stress at the fracture indicated improved flexure strength in the electrolytes with layered designs at both temperatures. It is believed to be the result of the residual compressive stress in the outer YSZ layer. In addition, the Weibull statistics of the stress at the fracture at room temperature was studied, and the values of residual stress presented at the outer layer were well verified.     

Thermal shock resistance and hoop strength of triplex silicon carbide composite tubes

Multi‐layered SiC composites have been considered as a nuclear fuel cladding material of light water reactors, LWRs, because of their excellent high temperature strength and corrosion resistance under accident conditions. During a design basis accident of a LWR such as a loss‐of‐coolant accident, the peak temperature of the fuel clad rapidly increases as the production of decay heat continues. The emergency core cooling systems then automatically supply the reactor core with emergency cooling water. The fuel clad consequently suffers from thermal shock. In this study, the structural integrity of multi‐layered SiC composite tubes after thermal shock was investigated. Several kinds of multi‐layered SiC composite tubes consisting of CVD SiC and CVI SiC_f/SiC were water‐quenched from 1200°C to room temperature. The triplex SiC composite tube retained its tubular geometry during quenching. The strength degradation after thermal shock was <13% for the specimens with a PyC interphase. The residual stress distribution within the tubes during thermal shock was evaluated by a finite element method.     

Effect of thermal residual stress on the tensile properties and damage process of C/SiC composites at high temperatures

Due to the mismatch of the thermal expansion coefficients between the matrix and yarns, thermal residual stress will appear in C/SiC composites. In this paper, a progressive damage model was used to predict the thermal-mechanical behavior of C/SiC composites and reveal the failure mechanism. Firstly, the properties of the composites under tensile load were tested at three different temperatures in vacuum. Then, the elastic-plastic progressive damage constitutive laws were used and implemented by a user-defined subroutine UMAT in ABAQUS. The thermal residual stress evolution in the cooling and heating processes was characterized. Finally, the stress-strain curves of the composites under tensile load at different temperatures were studied. The effects of thermal residual stress on the tensile properties and progressive damage process of C/SiC composites were revealed sequentially. This work can give design guidance for strengthening of C/SiC composites.     

Effects of residual stresses on the fracture properties of non-oxide laminated composites

A layered ceramic composite in the AlN–SiC–MoSi₂ system was prepared with the outer layers under residual compressive stress. The mechanical properties of the constituent layers and of the laminated composite were measured. Due to the residual compressive stress, the fracture strength of the laminated composite was higher than the strength of the outer layer material. The fracture toughness of the laminar composite was evaluated by SEVNB. The resulting values were compared with a fracture mechanics model and a good agreement was found between the experimental measurements and the calculated apparent fracture toughness profile.     

Effect of recoating slurry compositions on the microstructure and properties of SiC reticulated porous ceramics

Silicon carbide reticulated porous ceramics (SiC RPCs) were fabricated by polymer sponge replica technique, followed by recoating with SiC slurries of two different sintering additives of MgO–Al₂O₃–SiO₂ (Slurry 1) and polycarbosilane (Slurry 2). The sintering temperature of SiC RPCs recoated with Slurry 2 was 1100 °C, which was 200 °C lower than that for one recoated with Slurry 1. The prepared SiC RPCs exhibited homogeneous microstructure and contained pores with different sizes which was entrapped in the strut of SiC RPCs, small pores with diameter lower than 4 μm and large pores with diameter higher than 10 μm. Bending strength of SiC RPCs recoated with Slurry 1 was two times higher than that for the non-recoated samples, which was 1.88 MPa and was a little higher than that for one recoated with slurry 2. At the same time, high thermal shock resistance and high refractoriness were achieved for SiC RPCs recoated with Slurry 2.     

Fabrication of 2D C/ZrC–SiC composite and its structural evolution under high-temperature treatment up to 1800 °C

Two-dimensional C/ZrC–SiC composites were fabricated by chemical vapor infiltration (CVI) process combined with a modified polymer infiltration and pyrolysis (PIP) method. Two kinds of ZrC slurries (ZrC aqueous slurry and ZrC/polycarbosilane slurry) were employed to densify composites before the PIP process. The as-produced C/ZrC–SiC composites exhibited better mechanical properties than the C/SiC composites densified only by CVI and PIP process. Structural evolution for C/ZrC–SiC composites treated in the range 1200–1800 °C mainly consisted of the change of SiC whiskers and the decomposition of polymer derived ceramic.     

Fatigue of three advanced SiC/SiC ceramic matrix composites at 1200°C in air and in steam

High‐temperature mechanical properties and tension‐tension fatigue behavior of three advanced SiC/SiC composites are discussed. The effects of steam on high‐temperature fatigue performance of the ceramic‐matrix composites are evaluated. The three composites consist of a SiC matrix reinforced with laminated, woven SiC (Hi‐Nicalon?) fibers. Composite 1 was processed by chemical vapor infiltration (CVI) of SiC into the Hi‐Nicalon? fiber preforms coated with boron nitride (BN) fiber coating. Composite 2 had an oxidation inhibited matrix consisting of alternating layers of silicon carbide and boron carbide and was also processed by CVI. Fiber preforms had pyrolytic carbon fiber coating with boron carbon overlay applied. Composite 3 had a melt‐infiltrated (MI) matrix consolidated by combining CVI‐SiC with SiC particulate slurry and molten silicon infiltration. Fiber preforms had a CVI BN fiber coating applied. Tensile stress‐strain behavior of the three composites was investigated and the tensile properties measured at 1200°C. Tension‐tension fatigue behavior was studied for fatigue stresses ranging from 80 to 160 MPa in air and from 60 to 140 MPa in steam. Fatigue run‐out was defined as 2 × 10⁵ cycles. Presence of steam significantly degraded the fatigue performance of the CVI SiC/SiC composite 1 and of the MI SiC/SiC composite 3, but had little influence on the fatigue performance of the SiC/SiC composite 2 with the oxidation inhibited matrix. The retained tensile properties of all specimens that achieved fatigue run‐out were characterized. Composite microstructure, as well as damage and failure mechanisms were investigated.     

Improvement in the Strut Thickness of Reticulated Porous Ceramics

An improved technique has been developed for the successful fabrication of reticulate porous ceramics (RPCs) with strong struts, using polyurethane sponge as the template. In this technique, the coating process is composed of two stages. In the first stage, a thicker slurry is used to coat the sponge substrate uniformly. The green body is preheated to produce a reticulated preform with sufficient handling strength after the sponge has been burned out. In the second stage, a thinner slurry is used to coat the preform repeatedly, so that that struts are greatly thickened. Furthermore, large flaws, such as longitudinal strut cracks, are eliminated by the recoating process. The mechanical properties of RPCs should be improved significantly by this technique, which will make this material conducive for use in new technological applications.     

C/SiC composite-Ti6Al4V joints brazed with negative thermal expansion ZrP2WO12 nanoparticle reinforced AgCu alloy

Brazing C/SiC composites to Ti6Al4V alloy is associated with the problem of high residual stress inducing low joining strength. To overcome this problem, negative thermal expansion Zr₂P₂WO₁₂ (ZWP) nanoparticles were introduced into AgCu brazing alloy to obtain robust C/SiC-Ti6Al4V joints. Microstructures and mechanical properties of the joints brazed with different ZWP contents were investigated. Results indicated that 3 wt% ZWP nanoparticles dispersed homogeneously among brazing seam and compatible with brazing alloy. The width of reaction layer at C/SiC side was reduced sharply. Meanwhile, the finite element analysis showed that residual stress was reduced by 52.9 MPa and stress concentration among reaction layer was eliminated. The average shear strength of the joints brazed with AgCu + 3 wt% ZWP increased to 146.2 MPa, which was 70.8% higher than that of joints brazed without ZWP.     

Design,fabrication and properties of layered SiC/TiC ceramic with graded thermal residual stress

The finite element method (FEM) was used to design a symmetrical layered SiC/TiC ceramic with gradual thermal residual stress distribution. In the final model ceramic, the sequence of layers, from surface to inside, was SiC, SiC+2 wt.% TiC (S2T), SiC+4 wt.% TiC (S4T), SiC+6 wt.% TiC (S6T), SiC+8 wt.% TiC (S8T), and SiC+10 wt.% TiC (S10T); the thickness ratio of SiC:S2T:S4T:S6T:S8T:S10T was 1:1:1:1:1:10. After the model ceramic had been cooled from assumed sintering temperature 1850–20 °C in FEM calculation, gradual thermal residual stress, varying from surface compressive stress to inner tensile stress, was introduced. The designed ceramic then was fabricated by aqueous tape casting, stacking and hot-press sintering at 1850 °C, under 35 MPa pressure, for 30 min. The surface stress conditions of the sintered ceramic were tested by X-ray stress analysis, and those results were very close to the results from the FEM calculations. Compared with pure SiC and S10T ceramics fabricated by the same process, the designed ceramic showed excellent mechanical properties. The tested strength was close to the theoretical value. The strengthening and toughening mechanisms of the ceramic were ascribed to surface compressive residual stress.     

Multi‐scale hybrid composites‐based carbon nanotubes

Since the carbon nanotubes (CNTs) have been discovered, there has been a marked increase in the scientific literature dealing with multi‐scale composites. The multi‐scale hybrid composites with CNTs could endow the composites with some superior mechanical properties, such as improving the tensile performance, modest increasing compressive and flexural properties, and significantly enhancing interlaminar, interfacial and fracture strength. In addition, composites with CNTs can also develop the functional properties. A small quantity of CNTs can significantly increase the electrical properties of composites and lower the coefficient of thermal expansion of composites. The purpose of this work is to review the available literature in mechanical and functional properties of multi‐scale hybrid composites manufactured using CNTs. POLYM. COMPOS., 2011. © 2010 Society of Plastics Engineers     

Strengthening the thermal Negative Poisson's ratio structures by SiC chemical vapor infiltration

Negative Poisson's ratio structures exhibit adjustable thermal expansion behavior as the thermal stress can be dispersed or offset by torsion, bending, and tension of the struts. However, the structural stability under cyclic thermal stress significantly determines the long-term durability. Strengthening the Negative Poisson's ratio structure can ensure high thermal and mechanical reliability. The work designed a heat-induced torsional Negative Poisson's ratio structures and fabricated it by 3D printing. For efficient strengthening, the preforms were further densified by chemical vapor infiltration (CVI) of SiC to enhance the reliability. Pores and gaps in the preforms were homogeneously covered and filled by the SiC, enhancing the surface finish and mechanical performance. The heat induced torsion of the structures dispersed the heat flow in one single direction, reducing the thermal stress concentration. The independent thermal expansion change of the structural unit can offset or consume the heat dissipation stress, and further improve the reliability and thermal stability through the densification process. As a result, the 120° twisted structure exhibited an average coefficient of thermal expansion (CTE) of 6. 12 × 10^?6/K from room temperature (RT) to 500 °C, and the instantaneous CTE reached the minimum value of 4.01 × 10^?6/K at 125 °C. Meanwhile, the load-bearing capacity strengthened significantly, exhibiting the optimized strength of 11.31 MPa and Young's Modulus of 36.44 GPa, revealing a significant improvement than those of preforms, promising for high load-bearing and low expansion application of structure-function integrated low expansion material.     

Effect of oxidation and residual stress on mechanical properties of SiC seal coated C/SiC composite

The effect of oxidation and thermal residual stress on mechanical properties of SiC seal coated C/SiC composite at ambient temperature and high temperature were studied. The oxidation of SiC seal coated C/SiC composite at 1300 and 1500 °C resulted in carbon fibres burn area near through thickness micro cracks in the SiC seal coating. With the increase in exposure time, the formation of SiO₂ layer in SiC matrix near carbon fibres burns area was found. Residual mechanical properties of SiC seal coated C/SiC composite after exposure in air show significant degradation. First time, a continuous measurement of Young's modulus with temperature of C/SiC composite was carried out using an impulse excitation technique. The effect of relaxation of thermal residual stress on mechanical properties was observed with the help of continuous measurement of Young's modulus as a function of temperature in an inert atmosphere.